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(a) When would you use split, split less, or on-column injection in gas chromatography?

(b) Explain how solvent trapping and cold trapping work in split less injection.

Short Answer

Expert verified

(a.) Split injection is recommended if the sample contains >0.1% of the analyses of interest

(b.) In solvent trapping, the solvent condenses at the start of the column because the initial column temperature is set40C below the boiling point of the solvent. Solutes are then confined in the solvent as they catch up with the condensed plug of solvent.

Cold trapping is another technique of condensing solutes in a narrow band at the beginning of the column.

Step by step solution

01

To find the use split, split less, or on-column injection in gas chromatography

(a)

Split injection is recommended if the sample contains >0.1% of the analyses of interest Meanwhile, split less injection is applied for samples that has less than 0.01%analyses and requires trace analysis. Lastly, for samples that decay above their boiling points, on-column injection is preferred. It is also recommended for quantitative analysis.

02

finding the solvent trapping and cold trapping work in split less injection

(b)

In solvent trapping, the solvent condenses at the start of the column because the initial column temperature is set 40Cbelow the boiling point of the solvent. Solutes are then confined in the solvent as they catch up with the condensed plug of solvent. This method results to sharp chromatographic peaks, wherein the first peaks of interest should have boiling points 30 C greater than that of the solvent. The chromatography in solvent trapping starts when the column temperature is increased to vaporize the solvent trapped at the column head.

Cold trapping is another technique of condensing solutes in a narrow band at the beginning of the column. In this method, the initial column temperature is set at 150C lower than the boiling temperature of the solutes being considered. The solutes with high boiling points are trapped in a narrow band at the start of the column, while the solvent and components with low boiling points are quickly removed.

Chromatography of the high-boiling solutes is initiated by rapidly heating the column. Meanwhile, for low-boiling solutes, cryogenic focusing is needed and the initial column temperature is set below room temperature.

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Most popular questions from this chapter

When 1.06 mmol of 1-pentanol and 1.53 mmol of 1-hexanol were separated by gas chromatography, they gave peak areas of 922 and 1570 units, respectively. When 0.57 mmol of pentanol was added to an unknown containing hexanol, the peak areas were 843:816 (pentanol:hexanol). How much hexanol did the unknown contain?

3. (a) What are the advantages and disadvantages of using a narrower open tubular column?

(b) What are the advantages and disadvantages of using a longer open tubular column?

(c) What are the advantages and disadvantages of using a thicker film of stationary phase?

This problem reviews concepts from Chapter 23 using

Figure 24-7.

(a) Calculate the number of theoretical plates (N in Equation 23-30)

and the plate height (H) for CO.

(b) Find the resolution (Equation 23-23) between argon and oxygen.

(a) When a solution containing234mg of pentanol (FM 88.15) and237mg of 2,3 -dimethyl-2-butanol (FM 102.17) in10.0ml was separated, relative peak areas were pentanol: 2,3 -dimethyl-2-butanol = 0.913 : 1.00. Considering pentanol to be the internal standard, find the response factor for 2,3 -dimethyl-2-butanol.

(b) Use Equation 24-8 to find the areas for pentanol and 2,3 -dimethyl-2-butanol in Figure 24-8.

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Nitric oxide (NO) is a cell-signaling agent in physiologic processes including vasodilation, inhibition of clotting, and inflammation. A sensitive chromatography-mass spectrometry method was developed to measure two of its metabolites, nitrite(NO-2)and nitrat(NO3),in biological fluids. Internal standards,NO-152and15NO-3, were added to the fluid at concentrations of 80.0 and, respectively.Natural14NO-2and14NO-3plus the internal standards were then converted to volatile derivatives:

Because biological fluids are so complex, the derivatives were first isolated by high-performance liquid chromatography. For quantitative analysis, liquid chromatography peaks corresponding to the two products were injected into a gas chromatograph, ionized by negative ion chemical ionization (giving major peaks forNO-2andNO3-and the products measured by selected ion monitoring. Results are shown in the figure on the next page. If the internal standards undergo the same reactions and same separations at the same rate as theN14analytes, then the concentrations of analytes are simply[14NOx-]=[15NOx-](R-Rblank)

where R is the measured peak area ratio(m/z46/47fornitriteandm/z62/63fornitrite)for nitrite andfor nitrate) andRblankis the measured ratio of peak areas in a blank prepared from the same buffers and reagents with no added nitrite or nitrate. The ratios of peak areas areand. The ratios for the blank werem/z46/47=0.062andm/z62/63=0.058. Find the concentrations of nitrite and nitrate in the urine.


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